EP1093872A1 - Controlling grain spacing in directional solidified castings - Google Patents

Controlling grain spacing in directional solidified castings Download PDF

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Publication number
EP1093872A1
EP1093872A1 EP00309255A EP00309255A EP1093872A1 EP 1093872 A1 EP1093872 A1 EP 1093872A1 EP 00309255 A EP00309255 A EP 00309255A EP 00309255 A EP00309255 A EP 00309255A EP 1093872 A1 EP1093872 A1 EP 1093872A1
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Prior art keywords
grain
starter
grains
casting
mold
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EP00309255A
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German (de)
French (fr)
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EP1093872B1 (en
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Michael Francis Xavier Gigliotti, Jr
Roger John Petterson
Shyh-Chin Huang
Lee Cranford Perocchi
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General Electric Co
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General Electric Co
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22DCASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D1/00Treatment of fused masses in the ladle or the supply runners before casting
    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B11/00Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
    • C30B11/14Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method characterised by the seed, e.g. its crystallographic orientation
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22DCASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D21/00Casting non-ferrous metals or metallic compounds so far as their metallurgical properties are of importance for the casting procedure; Selection of compositions therefor
    • B22D21/02Casting exceedingly oxidisable non-ferrous metals, e.g. in inert atmosphere
    • B22D21/025Casting heavy metals with high melting point, i.e. 1000 - 1600 degrees C, e.g. Co 1490 degrees C, Ni 1450 degrees C, Mn 1240 degrees C, Cu 1083 degrees C
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22DCASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D27/00Treating the metal in the mould while it is molten or ductile ; Pressure or vacuum casting
    • B22D27/04Influencing the temperature of the metal, e.g. by heating or cooling the mould
    • B22D27/045Directionally solidified castings
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22DCASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D27/00Treating the metal in the mould while it is molten or ductile ; Pressure or vacuum casting
    • B22D27/20Measures not previously mentioned for influencing the grain structure or texture; Selection of compositions therefor
    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B11/00Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/10Inorganic compounds or compositions
    • C30B29/52Alloys

Definitions

  • the invention relates to a method for controlling grain spacing of a columnar superalloy casting.
  • a superalloy includes nickel, cobalt, nickel-iron or iron-based heat resistant alloys that have superior strength and oxidation resistance at high temperatures.
  • the superalloy can contain chromium to impart surface stability and one or more minor constituents, such as molybdenum, tungsten, columbium, titanium or aluminum, for strengthening purposes.
  • the physical properties of a superalloy make it particularly useful for the manufacture of a gas turbine component.
  • a grain is an individual crystal in a polycrystalline solid.
  • a grain boundary is an interface between individual crystals.
  • the crystal grain characteristics of a superalloy can determine superalloy properties. For example, the strength of a superalloy is determined in part by grain spacing. At low temperatures, grain boundaries impede dislocation motion. Hence, fine grain equal axial structures are preferred for low temperature applications. At high temperatures, deformation processes are diffusion controlled. Diffusion along grain boundaries is much higher than within the grains. Hence, large-grain spacing structures can be stronger than fine grain structures in high temperature applications. Generally, failure originates at grain boundaries oriented perpendicular to the direction of an induced stress. By casting a superalloy to produce an elongated columnar structure with unidirectional crystals aligned substantially parallel to the long axis of the casting, the number of grain boundaries normal to the primary stress axis can be minimized.
  • Directional solidification is a method that is used for producing turbine blades and the like with columnar crystalline structures.
  • a crystalline growth structure is created at the base of a vertically disposed mold defining a part and a solidification front is propagated through the structure under the influence of a moving thermal gradient.
  • crystals of nickel, cobalt or iron-based superalloys are characterized by a "dendritic" morphology. Dendritic refers to a form of crystal growth where forming solid extends into still molten liquid as an array of fine-branched needles.
  • Cooling rate is the product of solidification rate and thermal gradient at a solid liquid interface.
  • Solidification rate kinetics vary with crystallographic orientation.
  • the solidification rate in nickel based superalloys is typically highest in the crystallographic unit cell edge direction ( ⁇ 100> direction).
  • One desired macrostructure of a directionally solidified superalloy consists of grains elongated along the direction of solidification so that grain boundaries are aligned in the solidification direction. It is further desired that the crystallographic unit cell edge direction ⁇ 100> of the grains be parallel to the solidification direction to provide improved mechanical properties. If two grains are growing side-by-side into a temperature gradient, the grain with growth axis closest to a ⁇ 100> direction grows faster. The faster growing grain also spreads laterally. Lateral spread of a grain occurs by growth of secondary arms. If two grains are growing side by side into a liquid, and one grain leads the other by secondary arm spacing, the leading grain will extend a secondary arm in front to pinch off the lagging grain.
  • the invention relates to a method of controlling grain spacing of a casting and to the product of the method.
  • a grain starter that is capable of nucleating a multiplicity of grains, is positioned within a mold.
  • the mold is filled with molten metal and a solidification interface is caused to pass from the grain starter through the molten metal by immersing the mold in a cooling bath to form a casting that has a multiplicity of grains nucleated by the grain starter.
  • a grain spacing is determined for a columnar article.
  • a grain starter is selected that has a grain spacing determined to provide the grain spacing in the article when the article is cast in a liquid metal cooled directional solidification process.
  • the grain starter is positioned in a mold and the mold is filled with molten metal.
  • a solidification interface is caused to pass from the grain starter through the molten metal by immersing the mold in a liquid metal cooling bath to form an article having a grain spacing determined by the grain starter spacing.
  • the invention in still another embodiment, relates to a method of producing a cast article with a substantially increased proportion of parallel axis grain structure.
  • the method comprises making a fine grain superalloy multicrystalline grain starter capable of nucleating a multiplicity of grains in a solidifying casting.
  • the grain starter is provided within a mold and the mold is filled with molten metal.
  • a solidification interface is then caused to pass from the grain starter through the solidifying casting by immersing the mold in a cooling bath to form a casting that has a multiplicity of grains nucleated by the grain starter.
  • a grain starter as embodied by the invention, is characterized by many, fine grains.
  • the grain starter is used at the base of a directionally solidified casting to assure emergence of ⁇ 100> grains.
  • the grain starter nucleates fine grains of all orientations. In all locations, there will be some grains with ⁇ 100> orientation.
  • the ⁇ 100> grains by competitive growth, pinch off the other orientations.
  • Figure 1 illustrates a casting produced by a liquid metal cooling process without use of the grain starter of the present invention.
  • the superalloy casting is made by pouring liquid metal into a mold or melting metal in situ.
  • a moving temperature profile is generated along the casting, for example by lowering the mold out of a furnace.
  • a few solid crystals nucleate from the liquid metal in the coldest region of the mold. These crystals are typically of random orientation.
  • the grains with nearest ⁇ 100> orientation pinch off the other grains.
  • This competitive growth process can result in misoriented grains that persist along the casting for considerable distance.
  • the casting may be deemed of poor quality and not useful for some applications.
  • a grain starter as embodied by the invention, is illustrated in Figure 2.
  • the grain starter has fine, randomly oriented grains. Randomly oriented grains result in crystalline growth characterized by many grains. In all regions, there will be a few grains with ⁇ 100> orientation. These ⁇ 100> grains are well-oriented grains that quickly pinch off growth of other grains.
  • a spacing of grain for the grain starter is less than the dendrite arm spacing of the casting. This permits ⁇ 100> oriented grains to establish first dendrite side arms that quickly pinch off growth of other grains.
  • the grain starter comprises a metal casting agent that is capable of nucleating fine grains in a superalloy.
  • the grain starter has a multiple crystalline structure comprising at least a multiplicity of grains.
  • the grain starter can be characterized by a grain spacing at least greater than about 10 PM.
  • Grain spacing of the grain starter can be chosen to be less than the anticipated dendritic arm spacing of the developing crystals. While dendritic arm spacing is a function of cooling rate, typically, the dendritic arm spacing is from about 10 ⁇ m up to about 500 ⁇ m, preferably from about 100 ⁇ m up to about 500 ⁇ m.
  • the grain spacing of the grain starter can be chosen to be less than about 500 ⁇ m, desirably less than about 200 ⁇ m, such as less than about 100 ⁇ m.
  • the required fine grain starters can be made by densification of at least one of a metal powder, a wrought metal, and a ceramic that is an efficient nucleating agent for fine grains.
  • the grain starter is made by mechanically working a bar of superalloy metal having a cast coarse grain size. The superalloy metal is plastically deformed, then annealed, or otherwise heat treated, to recrystallize the metal structure with a fine randomly oriented grain structure.
  • the superalloy in another process as embodied by the invention, can be mechanically worked, machined, or otherwise compounded at a low temperature, and then heat treated to recrystallize the metal to a final desired grain size.
  • a superalloy grain starter of undetermined grain structure is mechanically deformed and then placed in a directional solidification furnace mold.
  • the grain starter is used in an "as-worked" condition.
  • the grain starter can comprise nickel, chromium, or iron based superalloys.
  • grain starters include Hastelloy X, René 80, IN 738, Ni-20Cr-10Ti alloy, GTD-111, GTD-222, René 41, René 125, René 77, René 95, René 80, Inconel 706, Inconel 718, Inconel 625, cobalt-based HS188, cobalt-based L-605 and stainless steels.
  • Ceramic nucleating agents for fine grains in superalloys include, but are not limited to, cobalt oxide and cobalt aluminate.
  • a grain starter is advantageous for castings made by a liquid metal cooling process.
  • a mold In a directional solidification process, a mold is placed on a chill plate. Grains nucleate in a cold region as liquid metal is poured into the mold.
  • the mold In the liquid metal cooling process, the mold is lowered into a liquid metal for cooling. The mold is above the cooling bath at the beginning of solidification.
  • the grain starter can be used to assure proper grain nucleation as the metal cools.
  • Figure 3 illustrates a schematic sectional view of a furnace 10 for a directional solidification process, as embodied by the invention.
  • the directional solidification furnace 10 is heated, for example, by resistance heated graphite strips 12 within insulated furnace box 14.
  • a ceramic shell mold 16 is suspended in the furnace 10 by a mold positioner 19.
  • a grain starter 20 is disposed within the mold 16.
  • a superalloy 22 is melted in crucible 24 and poured through a basin 26 into the mold 16. Randomly oriented solid superalloy grains then nucleate on the grain starter 20. Mold 16 is then lowered into a liquid cooling metal 28 in a container 30 at a prescribed lowering rate. A solid-liquid interface advances upward in the liquid metal away from the cooling metal 28 as heat is carried away from the liquid metal by the cooling metal 28. An ingot is formed after the mold 16 is withdrawn from the furnace 10 and immersed into the cooling metal 28.
  • cylindrical castings were made in a Bridgman furnace using aluminum-based molds.
  • the furnace casting temperature is about 1550°C and withdrawal rate is about 12 inches/hour, and all dimensions and measurements are approximate.
  • Grain starters of sintered cobalt aluminate and of hot pressed nickel alloy René 80 are used as grain starters for nickel alloy GTD-111 castings.
  • the initial René 80 powder size is less than 500 ⁇ m.
  • the casting is lowered from the furnace and is cooled by radiation.
  • the furnace mold was provided with a cooling plate to simulate cooling by a cooling bath such as a liquid metal bath.
  • the composition of the nickel alloy René 80 in weight percent is: Ni with 9.5 Co, 14 Cr.
  • the composition of the nickel alloy GTD-111 in weight percent is: Ni, 9.5 C0, 14 Cr, 1.6 Mo, 3.8 W, 3.0 Al, 4.9 Ti, 2.8 Ta, 0.10 C, 0.12 B and 0.04 Zr.
  • a 7/8" diameter casting of GTD-111 is grown in an aluminum oxide mold.
  • the casting is sectioned longitudinally and etched with acid to reveal the casting grain structure. Grain boundaries at angles greater than about 20° to the growth direction were observed for 2" above the base of the casting.
  • a casting is made in a manner similar to Example 1, except that a grain starter of hot pressed René 80 powder is placed at the bottom of the casting mold.
  • the grain size of the pressed Rene 80 is less than 500 ⁇ m.
  • the resulting casting exhibits a region of very fine grains, less than 1/16" in diameter for a 1 ⁇ 2" length of the casting. Above this region of fine grains, the grain structure is columnar, with boundaries oriented less than 20° to the growth direction. The structure above the region of fine grains is useable.
  • the region of acceptable casting represents an increase in yield beyond the yield of Example 1.
  • a casting is made in a manner similar to that of Example 1, except that a grain starter of sintered cobalt aluminate (CoAl 2 O 4 ) is placed at the bottom of the casting.
  • This grain starter has 1/8" inch deep grooves machined on its surface to increase contact area of the grain starter with superalloy.
  • a 1 ⁇ 2" region at the base of the casting exhibits equiaxed grains. Above the region, columnar structure is present beginning at less than 1 ⁇ 2" from the casting bottom. The useable casting extends beyond the 1 ⁇ 2" length. The region of acceptable casting represents a substantial increase in yield beyond Example 1.

Abstract

A grain starter capable of nucleating a multiplicity of grains in a casting is positioned within a mold. The mold is filled with molten metal and a solidification interface is caused to pass from the grain starter through the molten metal by immersing the mold in a cooling bath to form a casting that has a multiplicity of grains nucleated by the grain starter.

Description

  • The invention relates to a method for controlling grain spacing of a columnar superalloy casting.
  • A superalloy includes nickel, cobalt, nickel-iron or iron-based heat resistant alloys that have superior strength and oxidation resistance at high temperatures. The superalloy can contain chromium to impart surface stability and one or more minor constituents, such as molybdenum, tungsten, columbium, titanium or aluminum, for strengthening purposes. The physical properties of a superalloy make it particularly useful for the manufacture of a gas turbine component.
  • A grain is an individual crystal in a polycrystalline solid. A grain boundary is an interface between individual crystals. The crystal grain characteristics of a superalloy can determine superalloy properties. For example, the strength of a superalloy is determined in part by grain spacing. At low temperatures, grain boundaries impede dislocation motion. Hence, fine grain equal axial structures are preferred for low temperature applications. At high temperatures, deformation processes are diffusion controlled. Diffusion along grain boundaries is much higher than within the grains. Hence, large-grain spacing structures can be stronger than fine grain structures in high temperature applications. Generally, failure originates at grain boundaries oriented perpendicular to the direction of an induced stress. By casting a superalloy to produce an elongated columnar structure with unidirectional crystals aligned substantially parallel to the long axis of the casting, the number of grain boundaries normal to the primary stress axis can be minimized.
  • Directional solidification is a method that is used for producing turbine blades and the like with columnar crystalline structures. Generally, a crystalline growth structure is created at the base of a vertically disposed mold defining a part and a solidification front is propagated through the structure under the influence of a moving thermal gradient. During directional solidification, crystals of nickel, cobalt or iron-based superalloys are characterized by a "dendritic" morphology. Dendritic refers to a form of crystal growth where forming solid extends into still molten liquid as an array of fine-branched needles. Spacing between the needles in the solidification direction is called "primary dendrite arm spacing." Spacing of side branches or arms along a needle's length is termed "secondary dendrite arm spacing." Both primary and secondary dendrite arm spacing are functions of cooling rate. Cooling rate is the product of solidification rate and thermal gradient at a solid liquid interface.
  • Solidification rate kinetics vary with crystallographic orientation. For a fixed driving force, the solidification rate in nickel based superalloys is typically highest in the crystallographic unit cell edge direction (<100> direction).
  • One desired macrostructure of a directionally solidified superalloy consists of grains elongated along the direction of solidification so that grain boundaries are aligned in the solidification direction. It is further desired that the crystallographic unit cell edge direction <100> of the grains be parallel to the solidification direction to provide improved mechanical properties. If two grains are growing side-by-side into a temperature gradient, the grain with growth axis closest to a <100> direction grows faster. The faster growing grain also spreads laterally. Lateral spread of a grain occurs by growth of secondary arms. If two grains are growing side by side into a liquid, and one grain leads the other by secondary arm spacing, the leading grain will extend a secondary arm in front to pinch off the lagging grain. This phenomenon is termed "competitive growth." Until competitive growth achieves a structure of only grains close to the <100> direction, the grain boundaries will not be parallel and along the axis of the cast part. The section of a casting where the grains are competing to establish parallel growth is unusable as a turbine part and must be discarded.
  • A need exists for a directional solidification process that can produce columnar castings characterized by prescribed grain spacings. Additionally, a need exists for a directional solidification process that provides an increased proportion of casting characterized by aligned parallel axis oriented crystals.
  • SUMMARY OF THE INVENTION
  • The invention relates to a method of controlling grain spacing of a casting and to the product of the method. In the method, a grain starter that is capable of nucleating a multiplicity of grains, is positioned within a mold. The mold is filled with molten metal and a solidification interface is caused to pass from the grain starter through the molten metal by immersing the mold in a cooling bath to form a casting that has a multiplicity of grains nucleated by the grain starter.
  • In an embodiment, a grain spacing is determined for a columnar article. A grain starter is selected that has a grain spacing determined to provide the grain spacing in the article when the article is cast in a liquid metal cooled directional solidification process. The grain starter is positioned in a mold and the mold is filled with molten metal. A solidification interface is caused to pass from the grain starter through the molten metal by immersing the mold in a liquid metal cooling bath to form an article having a grain spacing determined by the grain starter spacing.
  • In still another embodiment, the invention relates to a method of producing a cast article with a substantially increased proportion of parallel axis grain structure. The method comprises making a fine grain superalloy multicrystalline grain starter capable of nucleating a multiplicity of grains in a solidifying casting. The grain starter is provided within a mold and the mold is filled with molten metal. A solidification interface is then caused to pass from the grain starter through the solidifying casting by immersing the mold in a cooling bath to form a casting that has a multiplicity of grains nucleated by the grain starter.
  • BRIEF DESCRIPTION OF THE DRAWINGS
  • Figure 1 is a schematic representation of a microstructure with heteregeneous grain nucleation;
  • Figure 2 is a schematic representation of a microstructure growth from a fine-grain grain starter; and
  • Figure 3 is a schematic sectional view of a furnace for conducting a directional solidification process.
  • DETAILED DESCRIPTION OF THE INVENTION
  • According to the invention, A grain starter, as embodied by the invention, is characterized by many, fine grains. The grain starter is used at the base of a directionally solidified casting to assure emergence of <100> grains. The grain starter nucleates fine grains of all orientations. In all locations, there will be some grains with <100> orientation. The <100> grains, by competitive growth, pinch off the other orientations.
  • Figure 1 illustrates a casting produced by a liquid metal cooling process without use of the grain starter of the present invention. In Figure 1, the superalloy casting is made by pouring liquid metal into a mold or melting metal in situ. A moving temperature profile is generated along the casting, for example by lowering the mold out of a furnace. At the beginning of the solidification process, a few solid crystals nucleate from the liquid metal in the coldest region of the mold. These crystals are typically of random orientation. As directional solidification progresses, the grains with nearest <100> orientation pinch off the other grains. This competitive growth process can result in misoriented grains that persist along the casting for considerable distance. The casting may be deemed of poor quality and not useful for some applications.
  • A grain starter, as embodied by the invention, is illustrated in Figure 2. The grain starter has fine, randomly oriented grains. Randomly oriented grains result in crystalline growth characterized by many grains. In all regions, there will be a few grains with <100> orientation. These <100> grains are well-oriented grains that quickly pinch off growth of other grains. A spacing of grain for the grain starter is less than the dendrite arm spacing of the casting. This permits <100> oriented grains to establish first dendrite side arms that quickly pinch off growth of other grains.
  • The grain starter comprises a metal casting agent that is capable of nucleating fine grains in a superalloy. The grain starter has a multiple crystalline structure comprising at least a multiplicity of grains. The grain starter can be characterized by a grain spacing at least greater than about 10 PM. Grain spacing of the grain starter can be chosen to be less than the anticipated dendritic arm spacing of the developing crystals. While dendritic arm spacing is a function of cooling rate, typically, the dendritic arm spacing is from about 10µm up to about 500µm, preferably from about 100µm up to about 500µm. The grain spacing of the grain starter can be chosen to be less than about 500µm, desirably less than about 200µm, such as less than about 100µm.
  • The required fine grain starters can be made by densification of at least one of a metal powder, a wrought metal, and a ceramic that is an efficient nucleating agent for fine grains. In one process, the grain starter is made by mechanically working a bar of superalloy metal having a cast coarse grain size. The superalloy metal is plastically deformed, then annealed, or otherwise heat treated, to recrystallize the metal structure with a fine randomly oriented grain structure.
  • In another process as embodied by the invention, the superalloy can be mechanically worked, machined, or otherwise compounded at a low temperature, and then heat treated to recrystallize the metal to a final desired grain size.
  • In further process, as embodied by the invention, a superalloy grain starter of undetermined grain structure is mechanically deformed and then placed in a directional solidification furnace mold. The grain starter is used in an "as-worked" condition.
  • The grain starter can comprise nickel, chromium, or iron based superalloys. Examples of such grain starters include Hastelloy X, René 80, IN 738, Ni-20Cr-10Ti alloy, GTD-111, GTD-222, René 41, René 125, René 77, René 95, René 80, Inconel 706, Inconel 718, Inconel 625, cobalt-based HS188, cobalt-based L-605 and stainless steels. Ceramic nucleating agents for fine grains in superalloys include, but are not limited to, cobalt oxide and cobalt aluminate.
  • The use of a grain starter is advantageous for castings made by a liquid metal cooling process. In a directional solidification process, a mold is placed on a chill plate. Grains nucleate in a cold region as liquid metal is poured into the mold. In the liquid metal cooling process, the mold is lowered into a liquid metal for cooling. The mold is above the cooling bath at the beginning of solidification. The grain starter can be used to assure proper grain nucleation as the metal cools.
  • Figure 3 illustrates a schematic sectional view of a furnace 10 for a directional solidification process, as embodied by the invention. In Figure 3, the directional solidification furnace 10 is heated, for example, by resistance heated graphite strips 12 within insulated furnace box 14. A ceramic shell mold 16 is suspended in the furnace 10 by a mold positioner 19. A grain starter 20 is disposed within the mold 16.
  • A superalloy 22 is melted in crucible 24 and poured through a basin 26 into the mold 16. Randomly oriented solid superalloy grains then nucleate on the grain starter 20. Mold 16 is then lowered into a liquid cooling metal 28 in a container 30 at a prescribed lowering rate. A solid-liquid interface advances upward in the liquid metal away from the cooling metal 28 as heat is carried away from the liquid metal by the cooling metal 28. An ingot is formed after the mold 16 is withdrawn from the furnace 10 and immersed into the cooling metal 28.
  • These and other features will become apparent from the following examples. The examples are not intended to limit the invention in any way.
  • In the following examples, cylindrical castings were made in a Bridgman furnace using aluminum-based molds. In each example, the furnace casting temperature is about 1550°C and withdrawal rate is about 12 inches/hour, and all dimensions and measurements are approximate. Grain starters of sintered cobalt aluminate and of hot pressed nickel alloy René 80 are used as grain starters for nickel alloy GTD-111 castings. The initial René 80 powder size is less than 500 µm. In a conventional Bridgman furnace, the casting is lowered from the furnace and is cooled by radiation. In the following examples, the furnace mold was provided with a cooling plate to simulate cooling by a cooling bath such as a liquid metal bath. The composition of the nickel alloy René 80 in weight percent is: Ni with 9.5 Co, 14 Cr. 4.0 Mo, 4.0 W, 3.0 Al, 5.0 Ti, 0.17 C, 0.015 B and 0.03 Zr. The composition of the nickel alloy GTD-111 in weight percent is: Ni, 9.5 C0, 14 Cr, 1.6 Mo, 3.8 W, 3.0 Al, 4.9 Ti, 2.8 Ta, 0.10 C, 0.12 B and 0.04 Zr.
  • EXAMPLE 1
  • A 7/8" diameter casting of GTD-111 is grown in an aluminum oxide mold. The casting is sectioned longitudinally and etched with acid to reveal the casting grain structure. Grain boundaries at angles greater than about 20° to the growth direction were observed for 2" above the base of the casting.
  • EXAMPLE 2
  • A casting is made in a manner similar to Example 1, except that a grain starter of hot pressed René 80 powder is placed at the bottom of the casting mold. The grain size of the pressed Rene 80 is less than 500 µm. The resulting casting exhibits a region of very fine grains, less than 1/16" in diameter for a ½" length of the casting. Above this region of fine grains, the grain structure is columnar, with boundaries oriented less than 20° to the growth direction. The structure above the region of fine grains is useable. The region of acceptable casting represents an increase in yield beyond the yield of Example 1.
  • EXAMPLE 3
  • A casting is made in a manner similar to that of Example 1, except that a grain starter of sintered cobalt aluminate (CoAl2O4) is placed at the bottom of the casting. This grain starter has 1/8" inch deep grooves machined on its surface to increase contact area of the grain starter with superalloy. A ½" region at the base of the casting exhibits equiaxed grains. Above the region, columnar structure is present beginning at less than ½" from the casting bottom. The useable casting extends beyond the ½" length. The region of acceptable casting represents a substantial increase in yield beyond Example 1.
  • While embodiments of the invention have been described, the present invention is capable of variation and modification, and therefore should not be limited to the precise details of the examples. The invention includes changes and alterations that fall within the purview of the following claims.

Claims (21)

  1. A method of controlling grain spacing of a casting, the method comprising:
    positioning a grain starter capable of nucleating a multiplicity of grains in a solidifying casting within a mold;
    filling the mold with molten metal; and
    passing a solidification interface from the grain starter through the solidifying casting by immersing the mold in a cooling bath to form a casting that comprises a multiplicity of grains that are nucleated by the grain starter.
  2. The method of claim 1, wherein the grain starter comprises a grain spacing less than a desired dendrite arm spacing of the solidifying casting.
  3. The method of claim 1, wherein the grain starter comprises a grain spacing less than about 500µm.
  4. The method of claim 1, wherein the cooling bath comprises a liquid metal cooling bath.
  5. The method of claim 1, wherein the grain starter comprises a metal casting agent capable of nucleating fine grains in a superalloy.
  6. The method of claim 1, wherein the grain starter comprises densifying metal powder.
  7. The method of claim 1, wherein the grain starter is at least one of mechanically worked and heat treated wrought metal or ceramic.
  8. The method of claim 1, wherein the grain starter comprises nickel, chromium, iron based superalloy.
  9. The method of claim 1, wherein the casting comprises a superalloy and the grain starter comprises cobalt oxide or cobalt aluminate.
  10. The method of claim 1, wherein the grain starter comprises GTD-111 or Rene 80.
  11. The method of claim 1, wherein the casting comprises a superalloy and the grain starter comprises the same superalloy as the casting.
  12. The method of claim 1, wherein the casting comprises a gas turbine blade.
  13. A cast columnar article comprising a region of grains less than 1/16" in diameter extending less than 2 inches above a base of the article.
  14. The article of claim 13, wherein the region of grains less than 1/16" in diameter extends less than a 1/2" length above the base of the article.
  15. The article of claim 13, further comprising a columnar grain structure with boundaries less than 20° to the growth direction that extends above the region of grains less than 1/16" in diameter.
  16. A liquid metal cooled directional solidification method to form an article with a columnar grain spacing, the method comprising:
    determining a grain spacing for a columnar article;
    selecting a grain starter having a grain spacing that is sufficient to provide the grain spacing in the article when the article is cast by the liquid metal cooled directional solidification process;
    disposing the grain starter in a mold;
    filling the mold with molten metal; and
    passing a solidification interface from the grain starter through the molten metal by immersing the mold in the liquid metal cooling bath to form the article having a columnar-grained spacing determined by the grain starter spacing.
  17. A method of casting a single crystal columnar-grained article, the method comprising:
    providing a mold filled with molten metal and a grain starter;
    moving a solidification interface along an axis of the mold by immersing the mold into a liquid metal cooling medium to provide single crystal columnar-grained article with <100> grains substantially along the length of the single oriented columnar-grained article.
  18. A method of producing a cast article with a parallel axis grain structure, the method comprising:
    making a fine-grain superalloy multicrystalline grain starter capable of nucleating a multiplicity of grains in a solidifying casting;
    providing the grain starter within a mold;
    filling the mold with molten metal; and
    passing a solidification interface from the grain starter through the solidifying casting by immersing the mold in a cooling bath to form a cast article with a parallel axis grain structure comprising a multiplicity of grains nucleated by the grain starter.
  19. The method of claim 18, wherein the step of making the starter comprises:
    densifying a metal powder to form a structure having a coarse grain size;
    heat treating the structure to refine grain size within with randomly oriented multiple grains: and
    providing the structure as the grain starter.
  20. The method of claim 18, wherein the step of making the starter comprises:
    at least one of mechanically working, machining, and compounding one of a metal and ceramic to form a structure having deformed grains; and
    heating the structure to a temperature sufficient to recrystallize the structure to randomly oriented multiple grains;
  21. The method of claim 18, wherein the step of making the starter comprises:
       at least one of mechanically working, machining or compounding a metal or ceramic to form a starter having deformed grains.
EP00309255A 1999-10-22 2000-10-20 Controlling grain spacing in directional solidified castings Expired - Lifetime EP1093872B1 (en)

Applications Claiming Priority (2)

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US09/422,179 US6343641B1 (en) 1999-10-22 1999-10-22 Controlling casting grain spacing
US422179 1999-10-22

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EP1093872B1 EP1093872B1 (en) 2005-01-19

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7779890B2 (en) 1998-11-20 2010-08-24 Rolls-Royce Corporation Method and apparatus for production of a cast component
US8851151B2 (en) 1998-11-20 2014-10-07 Rolls-Royce Corporation Method and apparatus for production of a cast component
EP3842556A1 (en) * 2019-12-27 2021-06-30 Fundación Azterlan Inoculation process for grain refinement of a nickel base alloy

Families Citing this family (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1437426A1 (en) * 2003-01-10 2004-07-14 Siemens Aktiengesellschaft Process for producing single crystal structures
EP1561536A1 (en) * 2004-02-03 2005-08-10 Siemens Aktiengesellschaft Process of brazing repairing of a part having a base material with oriented microstructure
US20080257517A1 (en) * 2005-12-16 2008-10-23 General Electric Company Mold assembly for use in a liquid metal cooled directional solidification furnace
JP4528995B2 (en) * 2007-08-02 2010-08-25 国立大学法人東北大学 Method for producing Si bulk polycrystalline ingot
US20090314452A1 (en) * 2008-06-24 2009-12-24 Garlock Robert M Method of casting metal articles
US20100147481A1 (en) * 2008-12-15 2010-06-17 General Electric Company Methods of manufacturing casted articles, and systems
US9493357B2 (en) * 2011-11-28 2016-11-15 Sino-American Silicon Products Inc. Method of fabricating crystalline silicon ingot including nucleation promotion layer
JP6136210B2 (en) * 2012-11-21 2017-05-31 株式会社Ihi Mold, manufacturing method thereof, precision casting apparatus and precision casting method
DE102019110580A1 (en) * 2019-04-24 2020-10-29 Nemak, S.A.B. De C.V. Device and method for removing at least one cooling element from an at least partially demolded casting, method for introducing at least one cooling element into a mold core of a casting mold, cooling element and casting
US11859266B2 (en) * 2021-02-26 2024-01-02 Lawrence Livermore National Security, Llc Castable high temperature nickel-rare earth element alloys
TWI801846B (en) * 2021-04-21 2023-05-11 台灣雨虹有限公司 Unidirectional grain metals and its manufacturing process

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4108236A (en) * 1977-04-21 1978-08-22 United Technologies Corporation Floating heat insulating baffle for directional solidification apparatus utilizing liquid coolant bath
EP0126550A1 (en) * 1983-04-21 1984-11-28 Aeplc Casting articles by directional solidification
US4804311A (en) * 1981-12-14 1989-02-14 United Technologies Corporation Transverse directional solidification of metal single crystal articles
RU2010672C1 (en) * 1991-02-15 1994-04-15 Всероссийский научно-исследовательский институт авиационных материалов Method of producing monocrystalline castings

Family Cites Families (17)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3763926A (en) * 1971-09-15 1973-10-09 United Aircraft Corp Apparatus for casting of directionally solidified articles
US3972367A (en) 1975-06-11 1976-08-03 General Electric Company Process for forming a barrier layer on ceramic molds suitable for use for high temperature eutectic superalloy casting
US3955616A (en) 1975-06-11 1976-05-11 General Electric Company Ceramic molds having a metal oxide barrier for casting and directional solidification of superalloys
US4031945A (en) 1976-04-07 1977-06-28 General Electric Company Process for making ceramic molds having a metal oxide barrier for casting and directional solidification of superalloys
US4213497A (en) 1978-08-21 1980-07-22 General Electric Company Method for casting directionally solidified articles
US4202400A (en) 1978-09-22 1980-05-13 General Electric Company Directional solidification furnace
US4289570A (en) * 1978-12-13 1981-09-15 United Technologies Corporation Seed and method for epitaxial solidification
US4292076A (en) 1979-04-27 1981-09-29 General Electric Company Transverse ductile fiber reinforced eutectic nickel-base superalloys
IL65014A0 (en) 1981-03-02 1982-04-30 Trw Inc Method of casting an article
US4475582A (en) * 1982-01-27 1984-10-09 United Technologies Corporation Casting a metal single crystal article using a seed crystal and a helix
US4589937A (en) 1982-09-22 1986-05-20 General Electric Company Carbide reinforced nickel-base superalloy eutectics having improved resistance to surface carbide formation
US4813470A (en) 1987-11-05 1989-03-21 Allied-Signal Inc. Casting turbine components with integral airfoils
US5071054A (en) 1990-12-18 1991-12-10 General Electric Company Fabrication of cast articles from high melting temperature superalloy compositions
US5366695A (en) 1992-06-29 1994-11-22 Cannon-Muskegon Corporation Single crystal nickel-based superalloy
US5445688A (en) 1994-03-03 1995-08-29 General Electric Company Method of making alloy standards having controlled inclusions
US5858558A (en) 1996-10-30 1999-01-12 General Electric Company Nickel-base sigma-gamma in-situ intermetallic matrix composite
US6213192B1 (en) * 1998-12-15 2001-04-10 General Electric Company Large structural, thin-wall castings made of metals subject to hot tearing, and their fabrication

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4108236A (en) * 1977-04-21 1978-08-22 United Technologies Corporation Floating heat insulating baffle for directional solidification apparatus utilizing liquid coolant bath
US4804311A (en) * 1981-12-14 1989-02-14 United Technologies Corporation Transverse directional solidification of metal single crystal articles
EP0126550A1 (en) * 1983-04-21 1984-11-28 Aeplc Casting articles by directional solidification
RU2010672C1 (en) * 1991-02-15 1994-04-15 Всероссийский научно-исследовательский институт авиационных материалов Method of producing monocrystalline castings

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
DATABASE WPI Section Ch Week 199503, Derwent World Patents Index; Class M22, AN 1995-020454, XP002158050 *

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7779890B2 (en) 1998-11-20 2010-08-24 Rolls-Royce Corporation Method and apparatus for production of a cast component
US7824494B2 (en) 1998-11-20 2010-11-02 Rolls-Royce Corporation Method and apparatus for production of a cast component
US8082976B2 (en) 1998-11-20 2011-12-27 Rolls-Royce Corporation Method and apparatus for production of a cast component
US8087446B2 (en) 1998-11-20 2012-01-03 Rolls-Royce Corporation Method and apparatus for production of a cast component
US8181692B2 (en) 1998-11-20 2012-05-22 Rolls-Royce Corporation Method and apparatus for production of a cast component
US8851152B2 (en) 1998-11-20 2014-10-07 Rolls-Royce Corporation Method and apparatus for production of a cast component
US8851151B2 (en) 1998-11-20 2014-10-07 Rolls-Royce Corporation Method and apparatus for production of a cast component
EP3842556A1 (en) * 2019-12-27 2021-06-30 Fundación Azterlan Inoculation process for grain refinement of a nickel base alloy

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US6343641B1 (en) 2002-02-05
EP1093872B1 (en) 2005-01-19
KR100718405B1 (en) 2007-05-14
KR20010040128A (en) 2001-05-15
JP2001246457A (en) 2001-09-11
DE60017523D1 (en) 2005-02-24

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